Device for sampling liquids from vacuum operating equipments

ABSTRACT

A device for sampling liquids from reaction equipments and particularly from vacuum operating reaction equipments, comprising a body fixedly secured to the bottom of the equipment and having an outlet duct fitting with a check valve, which movable component is kept closed by the atmospheric pressure. A movable assembly, comprising a sampling container and a feeding duct therefor, may be sealingly connected with said body in such a manner as to mechanically control the engagement of said check valve movable component with a related seat, means being provided to reach a given vacuum value in said container and said feeding duct.

United States Patent inventors Appl. No. Filed Patented AssigneePriority Francesco Sidari;

Franco Magnoni; Battista Morandi, all of Cesano Maderno, Milan, ItalyDec. 1 1, i969 Aug. 10, I97 1 Snh Viscose Societa Nazionale lndustriaApplicazioni Viscosa Milan, Italy Dec. 30, 1968 Italy DEVICE FORSAMPLING LIQUIDS FROM VACUUM OPERATING EQUIPMENTS 7 Claims, 4 DrawingFigs.

0.8. CI. 73/422 R Int. Cl. G0ln 1/14 Field of Search 73/422 R, 421 B[56] References Cited UNITED STATES PATENTS 2,844,964 7/1958 Guibert73/422 3,308,669 3/1967 Grise et al 73/422 Primary Examiner- Louis R.Prince Assistant Examiner-William A. Henry, ll Attorney-Wenderoth, Lindand Ponack ABSTRACT: A device for sampling liquids from reactionequipments and particularly from vacuum operating reaction equipments,comprising a body fixedly secured to the bottom of the equipment andhaving an outlet duct fitting with a check valve, which movablecomponent is kept closed by the atmospheric pressure. A movableassembly, comprising a sampling container and a feeding duct therefor,may be sealingly connected with said body in such a manner as tomechanically control the engagement of said check valve movablecomponent with a related seat, means being provided to reach a givenvacuum value in said container and said feeding duct.

Patented Aug. 10, 1971 FRANCESCF) SICLART FRANCO MAK NONI a:-

Attorr :ys

' DEVICE, FOR SAMPLING LI UIDs FROM VACUUM OPERATING EQUIPMENTS.BAckoRoUND This inventionconcerns a device adapted to be structurallyand v operatively associated with vacuum or low-pressure operatingequipments, for sampling liquid products or compounds contained, or evenprocessed therein.

The device according to the invention is particularly adapted to beassociated with polymerization reaction vessels and like equipments ofthe chemical industry, any other suitable application being howeverforeseen, under conditions conand even temporarily reset the atmosphericpressure in the environment must be excluded. 1

Such sampling operations have been heretofore carried out withdifficulty by means ofso-called syringes or by means of expensive andcomplex devices, wherein is very difficult to maintain a vacuum higherthan that existing in the processing environment downstream the passagethrough which the liquid is sampled. Moreover, theuse of check valves,which automatically open when a given vacuum value is attained at thedownstream, side, is often inadequate, since the valve movablecomponents open by themselves, owing to gravity forces or other reasons,before a vacuum higher than that exlsting at the upstream side isattained at the downstream side.

SUMMARY An object this invention is to provide a device, having anunusually simple design, adapted to operate under the most convenientworking conditions and wherein the restrictions and drawbacks of theheretofore known devices are, obviated. More detailedly, this inventionconcerns a device for sampling liquids from equipments that. operate ata subatmospheric pressure and practically under a high vacuum,comprising a component adapted to be permanently secured to said equipment, in particular but not necessarily to the bottom of the vacuumprocessing environment and including a valve system having a movablecomponent preferably in the form of a ball,. I j which operates tosealingly engage a seat formed at the end of xponent and designed to actas a control member, operable from the outside,'by which the valve ballcan be released from -said seat and 'the outlet passage can be openedwhen the required pressure conditions upstream and downstream saidpassage are attained.

DRAWINGS FlG. l is an exploded side view of'the main components of thedevice.

FIG. 2 is a side view, partly in a section on its symmetry plane, of'thedevice. as already fitted to the related equipment, and preset forcarrying out the first evacuation step at the downstream side.

FIG. 3 is a fragmentary longitudinal section of the device having apassage through which the sample is taken out, in its open conditions.

FIG. 4 is a cross section, taken on the plane lV-lV of FIGS. 1 and 2,ofthe removable portion of device.

PREFERRED EMBODIMENT As shown in the drawings, the device comprisesessentially three main assemblies, individually outlined in FIG. 1,i.e., a first assembly 10, that can be permanently secured, e.g., byscrew means, to the bottom wall 11 of a polymerization vessel or likeequipment; a second assembly 12, that can be engaged with said firstassembly under the conditions as stated later on; and a container 13,wherein the sample can be collected, that in the considered example isin the form of a small beaker or cup, made of a preferably transparentmaterial and showing a wall strength sufficient to stand against thepressure of the outer atmosphere, the latter components 12 and 13 beingable to cooperate with anyone of various assemblies 10, located e.g., indifferent positions, and/orjoined with different equipmerits.

Said assembly 10 comprises a firmly secured body 14, having a suitablepipefitting or connector 15, by which it can be fastened to said wall 11and through which a passage 16 is provided, having one end permanentlyin communication with the inside of the equipment, while its oppositeend leads into a small chamber 17, wherein a metal ball 18 is situated.Said ball defines a valve movable component and sealingly cooperateswith a supporting annular seat, that is formed on said end 19 (FIG. 3)of the passage 16, leading into the chamber 17. The best tight sealingconditions are thus ensured by the above arrangement, since a seal isobtained by a tight contact across a practically monodimensionalcircular line, whatever the orientation of the ball 18 may be.

An outside threaded portion 21 of a movable member 22 can be screwedinto an inside threaded connector 20, as formed on the bottom ofsaid'chamber 17. A noncircularly, e.g., polygonally shaped, portion 23of said movable member 22 extends below the fixed body 14, as it can beseen in FIG. 1.

A throughout passage 24, as formed inside the movable member 22 extendsupwardly through a-plurality of narrow channels 25 leading into saidchamber 17, the upper end of said member 22 acting as a rest means forthe ball 18, which can be thereby firmly forced against the seat 19 ofthe passage 16 by screwing upwardly said movable piece 22, as shown inFIG. 2. On the contrary, by loosening said member 22 relative to thefixed body 14., e.g., as shown in FIG. .3, the ball 18 is lifted out ofthe seat 19 and the passages 16 and 24 can communicate with each other.

The member 12 consists of an essentially tubular body, which upper endis formed with a flange 26 abutting against the bottom of the fixed bodyl4, said flange being externally shaped, e.g., with opposed facets 27,in such a manner as to allowa gripping action-therein for a rotationalmovement control, e.g., by a wrench. A tubular extension 28 dependingfrom said flange is formed with a flanged lower end 29, against whichthe upper edge 31 of a 'beaker 13 can be sealingly abutted, preferablyby means of an annular packing 30. Said bottom flange 29 is on turnpreferably formed with a passage 32, having a pipe duct 33, throughwhich the whole device can be connected to a vacuum pump, or other meansadapted to maintain a high vacuum below said flange and thus in thebeaker 13. The components 12 and 13 will be kept firmly engaged witheach other as in FIG. 2 as soon as a given vacuum value is attainedthrough thepassage 32. 4

As shownin particular in FIG. 4, a ring 34 is secured inside the upperend of the component 12, said ring comprising an inner wall shaped insuch a manner as to allow its engagement like a female wrench with saidportion 23 of the movable member 22 that .forms apart of thefixedassembly 10. Accordingly, when the different components are mutuallyengaged as'shown in FIG. 2, by acting from the outside, i.e., by

turning the component 12, a similar rotary motion can be imparted to themember 22, which is enclosed within the device, either to release theball 18 from its valve seat (FIG. 3), or to sealingly engage the sameagainst said seat, at the end of the passage 16.

The operation of the device according to the invention and theadvantages thereof become apparent from a consideration of the abovedescription and a comparative examination of the figures. When a sampleis to be taken out, then the components 12 and 13 are engaged with thestationary assembly 10, as shown in FIG. 2, whereafter the beaker 13 andthus all other components of the device located downstream the outlet oftee passage 16, are evacuated through the passage 32 until a vacuumhigher than that existing within the equipment is attained. At thistime, the valve ball 18 is removed from its seat by loosening thecomponent 12, whereby the liquid flows through the passages 16, 25, 24,and the sample is collected into the sampling beaker 13.

The liquid flowing-off can be stopped by screwing the component 12 intothe fixed assembly 10, until the ball is sealingly forced against itsseat 19. Then, the beaker 13 is vented to the atmosphere (or put incommunication with a source of a gas not affecting the sampled liquid),whereafter the components 12 and 13 can be removed from the fixedassembly and the sample can be taken out for a test.

Obviously, the ball 18 may be released even before a vacuum is appliedto beaker 13. In such a case, said ball acts like the movable componentof a check valve, and automatically opens when the downstream pressureis reduced down to a value sufficient to allow the ball 18 to falldownwardly under the combined action of the gravity force and of theupstream pressure. It is possible to conveniently follow said procedure,when a not too high vacuum is maintained within the equipment;obviously, the sample flowing-off will begin only when the downstreamvacuum is higher than the upstream one.

The device according to the invention has been previously describedunder the most typical operating conditions, i.e., for sampling liquidscontained inside of vacuum operated equipments, which obviously arethose requiring the overcoming of greatest difficulties and the solutionof specific technical problems.

However, the above-stated conditions do not represent a limitation ofthe range of application ofsaid device, which can be advantageouslyutilized also for sampling liquids from equipments operating at anatmospheric pressure, or even under pressure. Obviously, a greatimportance is to be attributed to this latter feature, which results ina greatly extended application range of said device, e.g., for takingout samples in any moment, in the course of processing wherein widelyvariable pressure conditions may exist, during the different stepsthereof.

Thus, when samples are to be taken out from pressure operatingequipments, an efficiently controlled valve is formed by the componentsof the assembly 10, since the ball 18, firmly pressed against the seat19 at the outlet of the passage 16, will ensure a tight sealing evenunder remarkably high pressures. By acting on the component 23, thevalve can be opened to allow a sample flowing through the passages 25and 24 and into the sampling container.

When the sampling is to carried out in a suitably conditionedenvironment, e.g., in a nitrogen atmosphere or the like, then thedifferent components as shown'in FIG. 1, or other equivalent ones, maybe associated e.g., as shown in H0. 2, in order to previously create andmaintain the nitrogen or other gas atmosphere in the passages and in thesampling container.

It is to be understood that the device according to the invention hasbeen described and shown as a nonrcstrictive example only, and thereforeit may be carried out by means ofdifferent structural solutions.

Thus, e.g., the sampling container 13, instead ofa beaker, as shown,might be in the form of a round-bottomed flask, preferably having acone-shaped frosted neck. Such flask should be adapted to tightly engagea tapered male connector formed e.g., by an extension of the component28, or also by the same component 28, which in this case is lacking theflange 29. The connector 32, 33 through which the air is evacuated andthe required atmosphere in the sampling container is created, may besecured to the upper end of the component 28, or it may be integral withthe round-bottomed flask or other sampling container.

Moreover the device may be completedwith other means, when necessary orconvenient, e.g., for heating some or all its components, e.g., forsampling products requiring to be kept at a given temperature forensuring a liquid condition thereof. The heating means may be in theform e.g., of electric resistances, pipe coils through which a heatingliquid or gas is circulated and the like, and such means may bestructurally associated and embodied in said components, when theparticular application of device requires a permanent or prevalentheating thereof.

It is therefore intended that all such changes, modifications andintegrations of device are covered by the present invention, inparticular as defined into one or more of the appended claims.

We claim:

1. A device for sampling liquids from vacuum operating equipments,comprising: a fixed assembly, designed to be permanently secured to theequipment and in particular to the bottom of the reaction environmentwherefrom the samples are to be taken out and having a passage fittedwith a check valve provided with a valve movable component arranged insuch a manner as to spontaneously, sealingly engage a related seat whenthe downstream pressure exceeds by a given, small value the upstreampressure inside the environment; a movable assembly, having a containerwherein the sample is collected, connection means for evacuating saidcontainer down to a vacuum higher than that existing within saidenvironment, means by which a tight connection with said seat in saidfixed assembly passage can be established, and means by which amechanical engagement with a member of said fixed assembly is providedand by which said valve movable component can be engaged with orreleased from said related seat, whereby when said assemblies areengaged with one another, said check valve can be opened and closed fromthe outside in order to control the start and the end of the sampleflowing into said container.

2. A device according to claim 1, wherein said valve movable componentis in the form ofa metal valve ball and said related seat is formed by acircular edge, whose diameter is smaller than that of said ball.

3. A device according to claim 1, wherein said fixed as sembly comprisesa movable components, in particular a screw-threaded component, which isconnected with the fixed portion wherein said valve seat is formed andabuts said valve movable component in order to force the same againstsaid valve seat, said components being formed with a noncircularshapedouter part adapted to torsionally engage a similarly shaped component,secured to said connection means of the movable assembly, whereby saidvalve movable component can be engaged and released by turning at leastone component ofsaid movable assembly.

4. A device according to claim 3, wherein said movable assemblycomprises a tubular components having a flanged upper end tightlyabutting against a stationary component of said fixed assembly, saidtubular component comprising means to establish a mechanical engagementwith said movable component designed to engage and release said valvemovable component, while the lower end of said tubular component isformed with a second flange against which the upper edge of a beaker orother sample collecting container can be tightly abutted.

5. A device according to claim 4, wherein said second flange is formedwith a passage leading below the same into said beakeror othercontainer, said passage being fitted with a pipe connection to a vacuumpump or other suitable means adapted to produce a vacuum, within saidbeaker or con- .t'ainer higher :ment. w

sembly is formedwith'an axially directed passage leading into saidprocessing environment and into a space wherein said valve movablecomponent is fitted. said assembly, below said space, being formed withan inner threaded part that engages with an outerthreaded part as formedinsaid movable component designed to engage andrelease said valvemovable components in respect of the outlet ofsaid passage,

said movable component is polygonally-shaped,-the upper end 'of saidnio'vable assembly .tubu lar component comprising a ring whichinneriside is correspondingly polygonally shaped, .whereby to act like awrench .when engaged with said polygonally shaped lower end ofsaid-movable component,

' thus allowing a rotational movement of said movable componentbyturning said movable assembly from outside.

7. Adevice accordingto claim 6, wherein theil o wer end of

1. A device for sampling liquids from vacuum operating equipments,comprising: a fixed assembly, designed to be permanently secured to theequipment and in particular to the bottom of the reaction environmentwherefrom the samples are to be taken out and having a passage fittedwith a check valve provided with a valve movable component arranged insuch a manner as to spontaneously, sealingly engage a related seat whenthe downstream pressure exceeds by a given, small value the upstreampressure inside the environment; a movable assembly, having a containerwherein the sample is collected, connection means for evacuating saidcontainer down to a vacuum higher than that existing within saidenvironment, means by which a tight connection with said seat in saidfixed assembly passage can be established, and means by which amechanical engagement with a member of said fixed assembly is providedand by which said valve movable component can be engaged with orreleased from said related seat, whereby when said assemblies areengaged with one another, said check valve can be opened and closed fromthe outside in order to control the start and the end of the sampleflowing into said container.
 2. A device according to claim 1, whereinsaid valve movable component is in the form of a metal valve ball andsaid related seat is formed by a circular edge, whose diameter issmaller than that of said ball.
 3. A device according to claim 1,wherein said fixed assembly comprises a movable component, in particulara screw-threaded component, which is connected with the fixed portionwherein said valve seat is formed and abuts said valve movable componeNtin order to force the same against said valve seat, said component beingformed with a noncircular-shaped outer part adapted to torsionallyengage a similarly shaped component, secured to said connection means ofthe movable assembly, whereby said valve movable component can beengaged and released by turning at least one component of said movableassembly.
 4. A device according to claim 3, wherein said movableassembly comprises a tubular component having a flanged upper endtightly abutting against a stationary component of said fixed assembly,said tubular component comprising means to establish a mechanicalengagement with said movable component designed to engage and releasesaid valve movable component, while the lower end of said tubularcomponent is formed with a second flange against which the upper edge ofa beaker or other sample collecting container can be tightly abutted. 5.A device according to claim 4, wherein said second flange is formed witha passage leading below the same into said beaker or other container,said passage being fitted with a pipe connection to a vacuum pump orother suitable means adapted to produce a vacuum, within said beaker orcontainer, higher than that existing in the processing environment.
 6. Adevice according to claim 3, wherein said fixed assembly is formed withan axially directed passage leading into said processing environment andinto a space wherein said valve movable component is fitted, saidassembly, below said space, being formed with an inner threaded partthat engages with an outer-threaded part as formed in said movablecomponent designed to engage and release said valve movable component inrespect of the outlet of said passage.
 7. A device according to claim 6,wherein the lower end of said movable component is polygonally shaped,the upper end of said movable assembly tubular component comprising aring which inner side is correspondingly polygonally shaped, whereby toact like a wrench when engaged with said polygonally shaped lower end ofsaid movable component, thus allowing a rotational movement of saidmovable component by turning said movable assembly from outside.